废旧印刷线路板热解油利用及轻质化研究
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摘要
现代社会,科技飞速发展,日新月异。各种家电设备、电子产品更新换代的周期越来越短,我们在享受最新科技成果给我们带来的便利同时,也不得不面对越来越多各类报废电子电器产品的处理处置问题。印刷线路板是各种电子电器产品中的重要零部件之一,也是现代城市中最典型的固体废弃物。废线路板具有种类繁多、数量巨大、增长迅速的特点。其主要成分为高分子有机树脂、铜等贵重金属、玻璃纤维。如果能将其中的组分尽数利用,不仅能带来巨大的经济效益,还能够切实减轻环境压力。在诸多废线路板处理工艺中,热解法处理废线路板能够将线路板中树脂、玻纤和铜完全剥离,对于后续各组分分别回收利用提供了很大的便利。但是,相较高价的铜和回收利用难度较低的玻璃纤维来说,废线路板热解油因为成分复杂,含有卤素阻燃剂等原因,回收利用难度较大,到目前为止,都没有学者提出比较好的利用方案。
本论文对将废线路板真空热解来制取热解油全组分利用工艺进行了研究,首先确定了废线路板制取热解油的最佳工艺条件。并利用大型分析仪器对热解油的成分进行分析。在了解了热解油成分的基础上,对热解油进行分馏,并探讨热解油较轻的液体组分合成热固性酚醛树脂的工艺。对于常温下呈固体的热解油重组分作为沥青改性剂利用的可行性。最后,本文还对热解过程中利用分子筛催化剂对热解油进行轻质化处理进行了系统研究。
首先,本文研究了废线路板制取热解油的最佳工艺。研究结果表明：在热解终温为550℃,升温速率为10℃/min,热解压力为20KPa,恒温时间为60min,物料尺寸为40mm×40mm时,有利于提高废线路板热解油的产率,降低固体和液体的产率。在该工艺条件下,液相产物可以达到18.6%,而固相产物达到76.1%,气相产物占5.3%。
接下来,将热解油进行常压实沸点蒸馏,并利用元素分析仪、气质联用仪、红外光谱分析仪对热解油各馏分进行测试。结果表明：热解油液体馏分主要集中在120℃-300℃温度段；各馏分以碳氢化合物为主,碳氢比在0.8上下,并含有少量S、N元素；热解油中含量最多的物质是苯酚、3-甲基、4-乙基苯酚,4-异戊基苯酚,4-异丙基苯酚,4、4,-亚乙基苯酚等物质,这类物质占到各馏分含量的60%以上；在红外图谱中,我们也看到了相应的羟基及苯环相关的峰。
在利用热解油轻组分合成热固性酚醛树脂的研究中,先利用L9(34)正交试验确定最佳工艺条件为：每38.5gWPCB轻组分、40g甲醛溶液、lOg NaOH、第一阶段温度60℃、第一阶段反应时间3h、第二阶段温度95℃、第二阶段反应时间3h。通过红外光谱、热重分析和力学性能测试发现：轻组分合成的热固性酚醛树脂出现CH2、CHOH等特征峰；轻组分酚醛树脂的固化分解温度为464.2℃,最终剩余质量为64.71%；轻组分酚醛树脂的拉伸强度能达到39.6Mpa,拉伸模量为8.8Gpa,与普通的热固性酚醛树脂的相关指标相仿。
在热解油重馏分改性沥青的研究中,我们发现热解油重馏分能够大幅度提升沥青的高温稳定性和路用性能。研究结果表明：以4%作为沥青中HFPO的最佳添加量时,改性沥青的软化点为53.1℃,针入度为72.4dmm,15℃下延度为43.3cm,在软化点指标上优于HFPO+SBR改性沥青和SBR改性沥青；重组分改性沥青混合料在油石比为5.0%时,马歇尔稳定度达到19.50,动稳定度可以达到10161次/mm,均高于HFPO+SBR沥青混合料和SBR改性沥青混合料。将重组分回收利用无论是从经济角度还是环境角度都是很有意义的。
利用分子筛催化剂对热解油进行轻质化,可以提高热解油的回收利用价值。该部分使用HZSM-5、USY、A12O3三种分子筛催化剂对废线路板进行催化热解。实验结果表明：HZSM-5热解液体产率最高；氧化铝将废线路板粉末分解最彻底；USY对三相产物产率影响较小。600℃时,A1203对热解油的轻质化效果最好,200℃以下轻组分含量最高,可达到56%；HZSM-5催化使热解油重组分含量减少了9%；USY轻质化效果不明显。在催化热解过程中,A1203能提高苯酚含量、并有一定的脱溴效果；HZSM-5和USY仅在一定程度上提高苯酚含量,未见明显脱溴效果。A1203能够减少热解油中的C15双环芳烃物质,使产物主要成分为C6和C9物质；而HZSM-5和USY对碳分布影响不大。
本论文研究成果填补了废线路板热解油的资源化利用的空白,为进一步推广废线路板热解处理工艺的工业化提供了理论指导。
In the nowadays of accelerating technology, product replacement begin to speed up. We have to face the problem on how to treat the waste electrical and electronic equipment (WEEE), although we are enjoying the convenient from the latest technology. Printed circuit boards are the one of the most important components. The increasing amount of waste electrical and electronic equipment is leading to a large amount of waste printed circuit boards (WPCBs). WPCB are also become the typical waste solid in modern cities. WPCB are characterized by wide range and enormous amount. WPCB consist of resins, copper, glass fiber, etc. If all of comonents are utilized, it can not only bring the significant economic benefits, but also protect the environment. Among the different type of methods in recycling WPCB, yrolysis has the advantage that all of the pyrolysis products (pyrolytic oil(PO), metals and glass fiber) can potentially be recovered and recycled. Compared with copper and glass fiber, PO is difficult in recycling due to its complexity of the components and halogen in fire retardant. Therefore, there is no mature method in recycling the PO from the pyrolysis of WPCB.
In this paper, the new method of recycling PO from WPCB was provided. Firstly, the optimal technological condition of preparing PO was determined. Then the PO was distillated into several fractions. All the liquid fractions were analyzed by element analyzer (EA), gas chromatoraph-mass spectrum (GC-MS), fourier transform-infrared spectroscopy (FT-IR). After that, the resource utilization on light fraction of PO (LFPO) and heavy fraction of PO (HFPO) were discussed. Finally, the effect on the light of PO in catalytic pyrolysis of WPCB was investigated.
From the experiment of pyrolysis, the productivity of PO was18.6%while the optimal technological conditions were the particle size of40mm×40mm, the pyrolysis temperature of550℃, the heating rate of10℃/min, the pyrolysis pressure of20kPa and the constant temperature time of60min. and the productivity of solid and gas were76.1%and5.3%.
After the true boiling point distillation (TBP) was carried. The major component was in120℃-300℃. All the fraction were analyzed by EA, GC-MS, FT-IR. The results showed that all the fractions consisted of over50%of C and6%of H. The C/H ratio of each fraction was0.8. Phenol and its substitutes were more than60%of pyrolytic oil. The spectrogram of the fractions of PO appeared characteristic peak such as CH2, CH-OH. Besides, less than10%of Br, which existed in bromophenolic compounds, was analysed in the pyrolytic oil.
Through the orthogonal experiment, the thermosetting phenolic resin was synthetized by using LFPO. The results showed that the optimal technological conditions were LFPO of38.5g, formaldehyde of40g. NaOH of lOg of the catalyst, the reaction temperature of60℃for3h,and then ramp to95℃for3h. The thermosetting phenolic resin was observed by FT-IR and thermogravimetry (TG-DTG). The results indicated that the peaks such as CH2. CH-OH were appeared. The product begins to solidify and decompose at464.2℃, the remaining quality is64.71%at last, which indicated that the product has a good heat resistance. In the test of The tensile strength of the phenolic resin was39.6Mpa and its tensile modulus is8.8Gpa, which indicated that the phenolic resin has a good mechanical properties.
In the field of using HFPO into modifying the asphalt, the The HFPO was tested as an asphalt modifier. Three asphalt modifiers were tested:HFPO; styrene-butadiene rubber (SBR); and HFPO+SBR (1:1). The physical properties and road performance of the three modified asphalts were measured and evaluated. The results have shown that when the amount of modifier was less than10%. the HFPO modified asphalt had the highest softening point of the three. HFPO+SBR modified asphalt did well in the test of penetration. SBR modified asphalt was good at the test of ductility. The dynamic stability (DS) and water resistance of the asphalt mixture with the HFPO modified asphalt was10161cycles/mm and87.2%, respectively. The DS was much larger than for the HFPO+SBR and SBR modified asphalt mixtures. These results indicate that using HFPO as an asphalt modifier has significant benefits not only for road engineering but also for resource recycling.
In the research on the catalytic pyrolysis of WPCB, HZSM-5, USY, A12O3was used as there type of catalysts. The results showed that the productivity of liquid was the highest when using HZSM-5as catalyst. The resins of WPCB could decompose completely. USY had little effect on the productivity of PO. When the reaction temperature of catalytic pyrolysis was600℃, A12O3showed the best performance in the light of PO. The fraction (<200℃) was56%; HFPO was decreased by9%by the addition of HZSM-5; but USY didn't show significant effect to the light of PO. A12O3had a dehalogen performance and in catalytic pyrolysis of WPCB. The results indicate that A12O3has a good performance in the light of PO and dehalogen. HZSM-5only do well in the light of PO. USY had little effect on the light of PO.
This research can not only fill the gap of recycling of PO from WPCB, but also provide the theoretical guidance for popularization of pyrolysis process of WPCB.
本论文对将废线路板真空热解来制取热解油全组分利用工艺进行了研究,首先确定了废线路板制取热解油的最佳工艺条件。并利用大型分析仪器对热解油的成分进行分析。在了解了热解油成分的基础上,对热解油进行分馏,并探讨热解油较轻的液体组分合成热固性酚醛树脂的工艺。对于常温下呈固体的热解油重组分作为沥青改性剂利用的可行性。最后,本文还对热解过程中利用分子筛催化剂对热解油进行轻质化处理进行了系统研究。
首先,本文研究了废线路板制取热解油的最佳工艺。研究结果表明：在热解终温为550℃,升温速率为10℃/min,热解压力为20KPa,恒温时间为60min,物料尺寸为40mm×40mm时,有利于提高废线路板热解油的产率,降低固体和液体的产率。在该工艺条件下,液相产物可以达到18.6%,而固相产物达到76.1%,气相产物占5.3%。
接下来,将热解油进行常压实沸点蒸馏,并利用元素分析仪、气质联用仪、红外光谱分析仪对热解油各馏分进行测试。结果表明：热解油液体馏分主要集中在120℃-300℃温度段；各馏分以碳氢化合物为主,碳氢比在0.8上下,并含有少量S、N元素；热解油中含量最多的物质是苯酚、3-甲基、4-乙基苯酚,4-异戊基苯酚,4-异丙基苯酚,4、4,-亚乙基苯酚等物质,这类物质占到各馏分含量的60%以上；在红外图谱中,我们也看到了相应的羟基及苯环相关的峰。
在利用热解油轻组分合成热固性酚醛树脂的研究中,先利用L9(34)正交试验确定最佳工艺条件为：每38.5gWPCB轻组分、40g甲醛溶液、lOg NaOH、第一阶段温度60℃、第一阶段反应时间3h、第二阶段温度95℃、第二阶段反应时间3h。通过红外光谱、热重分析和力学性能测试发现：轻组分合成的热固性酚醛树脂出现CH2、CHOH等特征峰；轻组分酚醛树脂的固化分解温度为464.2℃,最终剩余质量为64.71%；轻组分酚醛树脂的拉伸强度能达到39.6Mpa,拉伸模量为8.8Gpa,与普通的热固性酚醛树脂的相关指标相仿。
在热解油重馏分改性沥青的研究中,我们发现热解油重馏分能够大幅度提升沥青的高温稳定性和路用性能。研究结果表明：以4%作为沥青中HFPO的最佳添加量时,改性沥青的软化点为53.1℃,针入度为72.4dmm,15℃下延度为43.3cm,在软化点指标上优于HFPO+SBR改性沥青和SBR改性沥青；重组分改性沥青混合料在油石比为5.0%时,马歇尔稳定度达到19.50,动稳定度可以达到10161次/mm,均高于HFPO+SBR沥青混合料和SBR改性沥青混合料。将重组分回收利用无论是从经济角度还是环境角度都是很有意义的。
利用分子筛催化剂对热解油进行轻质化,可以提高热解油的回收利用价值。该部分使用HZSM-5、USY、A12O3三种分子筛催化剂对废线路板进行催化热解。实验结果表明：HZSM-5热解液体产率最高；氧化铝将废线路板粉末分解最彻底；USY对三相产物产率影响较小。600℃时,A1203对热解油的轻质化效果最好,200℃以下轻组分含量最高,可达到56%；HZSM-5催化使热解油重组分含量减少了9%；USY轻质化效果不明显。在催化热解过程中,A1203能提高苯酚含量、并有一定的脱溴效果；HZSM-5和USY仅在一定程度上提高苯酚含量,未见明显脱溴效果。A1203能够减少热解油中的C15双环芳烃物质,使产物主要成分为C6和C9物质；而HZSM-5和USY对碳分布影响不大。
本论文研究成果填补了废线路板热解油的资源化利用的空白,为进一步推广废线路板热解处理工艺的工业化提供了理论指导。
In the nowadays of accelerating technology, product replacement begin to speed up. We have to face the problem on how to treat the waste electrical and electronic equipment (WEEE), although we are enjoying the convenient from the latest technology. Printed circuit boards are the one of the most important components. The increasing amount of waste electrical and electronic equipment is leading to a large amount of waste printed circuit boards (WPCBs). WPCB are also become the typical waste solid in modern cities. WPCB are characterized by wide range and enormous amount. WPCB consist of resins, copper, glass fiber, etc. If all of comonents are utilized, it can not only bring the significant economic benefits, but also protect the environment. Among the different type of methods in recycling WPCB, yrolysis has the advantage that all of the pyrolysis products (pyrolytic oil(PO), metals and glass fiber) can potentially be recovered and recycled. Compared with copper and glass fiber, PO is difficult in recycling due to its complexity of the components and halogen in fire retardant. Therefore, there is no mature method in recycling the PO from the pyrolysis of WPCB.
In this paper, the new method of recycling PO from WPCB was provided. Firstly, the optimal technological condition of preparing PO was determined. Then the PO was distillated into several fractions. All the liquid fractions were analyzed by element analyzer (EA), gas chromatoraph-mass spectrum (GC-MS), fourier transform-infrared spectroscopy (FT-IR). After that, the resource utilization on light fraction of PO (LFPO) and heavy fraction of PO (HFPO) were discussed. Finally, the effect on the light of PO in catalytic pyrolysis of WPCB was investigated.
From the experiment of pyrolysis, the productivity of PO was18.6%while the optimal technological conditions were the particle size of40mm×40mm, the pyrolysis temperature of550℃, the heating rate of10℃/min, the pyrolysis pressure of20kPa and the constant temperature time of60min. and the productivity of solid and gas were76.1%and5.3%.
After the true boiling point distillation (TBP) was carried. The major component was in120℃-300℃. All the fraction were analyzed by EA, GC-MS, FT-IR. The results showed that all the fractions consisted of over50%of C and6%of H. The C/H ratio of each fraction was0.8. Phenol and its substitutes were more than60%of pyrolytic oil. The spectrogram of the fractions of PO appeared characteristic peak such as CH2, CH-OH. Besides, less than10%of Br, which existed in bromophenolic compounds, was analysed in the pyrolytic oil.
Through the orthogonal experiment, the thermosetting phenolic resin was synthetized by using LFPO. The results showed that the optimal technological conditions were LFPO of38.5g, formaldehyde of40g. NaOH of lOg of the catalyst, the reaction temperature of60℃for3h,and then ramp to95℃for3h. The thermosetting phenolic resin was observed by FT-IR and thermogravimetry (TG-DTG). The results indicated that the peaks such as CH2. CH-OH were appeared. The product begins to solidify and decompose at464.2℃, the remaining quality is64.71%at last, which indicated that the product has a good heat resistance. In the test of The tensile strength of the phenolic resin was39.6Mpa and its tensile modulus is8.8Gpa, which indicated that the phenolic resin has a good mechanical properties.
In the field of using HFPO into modifying the asphalt, the The HFPO was tested as an asphalt modifier. Three asphalt modifiers were tested:HFPO; styrene-butadiene rubber (SBR); and HFPO+SBR (1:1). The physical properties and road performance of the three modified asphalts were measured and evaluated. The results have shown that when the amount of modifier was less than10%. the HFPO modified asphalt had the highest softening point of the three. HFPO+SBR modified asphalt did well in the test of penetration. SBR modified asphalt was good at the test of ductility. The dynamic stability (DS) and water resistance of the asphalt mixture with the HFPO modified asphalt was10161cycles/mm and87.2%, respectively. The DS was much larger than for the HFPO+SBR and SBR modified asphalt mixtures. These results indicate that using HFPO as an asphalt modifier has significant benefits not only for road engineering but also for resource recycling.
In the research on the catalytic pyrolysis of WPCB, HZSM-5, USY, A12O3was used as there type of catalysts. The results showed that the productivity of liquid was the highest when using HZSM-5as catalyst. The resins of WPCB could decompose completely. USY had little effect on the productivity of PO. When the reaction temperature of catalytic pyrolysis was600℃, A12O3showed the best performance in the light of PO. The fraction (<200℃) was56%; HFPO was decreased by9%by the addition of HZSM-5; but USY didn't show significant effect to the light of PO. A12O3had a dehalogen performance and in catalytic pyrolysis of WPCB. The results indicate that A12O3has a good performance in the light of PO and dehalogen. HZSM-5only do well in the light of PO. USY had little effect on the light of PO.
This research can not only fill the gap of recycling of PO from WPCB, but also provide the theoretical guidance for popularization of pyrolysis process of WPCB.
引文
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